核磁共振波谱内标法测定四氯虫酰胺标样的含量

Quantitive Determination of Tetrachlorantraniliprole by 1H NMR Spectroscopy with Internal Standard Method

[目的]采用核磁共振波谱内标法,建立了快速、专属、准确测定四氯虫酰胺标样含量的方法。[方法]使用日本电子公司JNM-ECZ600R超导核磁共振波谱仪,以氘代二甲基亚砜为溶剂,顺丁烯二酸为内标,在测定温度25℃、脉冲宽度8.0μs、延迟时间为5 s、扫描次数8的条件下采集样品氢谱。[结果]以化学位移δ分别为10.55和6.27的四氯虫酰胺和顺丁烯二酸的氢质子峰作为定量峰,其峰面积比y(As/Ar)与质量比x(ms/mr)进行线性回归,相关系数为0.9999。含量测定重复性试验的RSD值为0.38%,稳定性的RSD值为0.77%,测得四氯虫酰胺标样的含量为99.6%。[结论]在没有标准对照品的情况下,核磁共振波谱法可用于四氯虫酰胺的含量测定,该方法具有快速、准确、简便的优点。

[Aims]This study aims to establish a rapid,specific and simple method for the quantitive determination of tetrachlorantraniliprole by 1H NMR.[Methods]1H NMR spectroscopy was acquired in DMSO,scanning 8 times at 25℃with a Jeol JNM-ECZ600R,pulses width 8.0μs,delay time 5 s,and maleic acid as internal standard.[Results]The integration of proton signals atδ10.55 for tetrachlorantraniliprole and atδ6.27 for maleic acid was used for quantification.The correlation coefficient was 0.9999 for quantitative peak areas ratio y(As/Ar)of tetrachlorantraniliprolemaleic acid versus mass ratio x(ms/mr).The precision RSD was 0.38%,the stability RSD was 0.77%.The contents of tetrachlorantraniliprole was 99.6%.[Conclusions]The results showed that 1H NMR method can be used for the quantative determination of tetrachlorantraniliprole with reference substance.The method is rapid,accurate and simple.